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APPLICATION NOTE

Metals in Sewage SludG™ – ERA 160

SUMMARY

The application note summarizes the digestion of ERA 160, a Metals in Sewage Sludge certified reference material using ColdBlock Digestion Pro Series Technology.

Instrument:

ColdBlock CBM, chiller, ICP-OES, ICP-MS (with CRC technology)

Published:March 2025
Digestion Time:45 Minutes
Acid Used:HNO3, HCl & H2O2
Average ColdBlock Recovery vs. CRM:
  • 107% Arsenic
  • 103% Mercury
  • 105% Selenium

METHODOLOGY

  1. Chiller temperature was set to -5°C
  2. 0.5g of each sample was weighed and placed into a ColdBlock Digestion vessel
  3. 10mL of 1:1 HNO3 + 5mL 1:1 HCl were added, and the samples were digested at 70% power for 5 minutes
  4. 10mL HNO3 was added and digested again at 60% power for 20 minutes (repeat this step if fuming continues)
  5. 3mL of 30% H2O2 was added slowly, and digested again at 60% for 10 minutes
  6. 5mL HCl was added and digested at 60% power for 10 minutes
  7. Samples were cooled and bulked to 50mL using ultrapure water

DISCUSSION

  • This method yielded data comparable to EPA 3050B standards in just 45 minutes
  • The addition of HCl in the final step of the digestion helps keep certain elements such as antimony and silver solubilized
  • This method is not appropriate for standard ICP-MS instruments that are not equipped with Collision/Reaction Cell technology

15 samples of ERA 160 after bulk up to 50mL

Results

ERA #160 Metals in Sewage SludG (lot:D122-160)

Method:

0.5g – Add 10mL 1:1 HNO3 + 5mL 1:1 HCl, digest at 70% for 5 minutes, then add 10mL HNO3 and digest at 60% for 20 minutes (repeat this step if fuming continues) Add 3mL of 30% H2O2, slowly and digest again @ 60% for 10 minutes, then add 5mL HCl and digest again @ 60% for 10 minutes. Cool and bulk to 50mL with ultrapure water

Element

*Reference Value (mg/kg) n=5

ColdBlock Average (mg/kg) n=16

ColdBlock Stdev

ColdBlock
% RSD

ColdBlock % Recovery vs SW-846 3050B

Aluminum

3228

3427

42.10

1.2%

106%

Antimony

108

124

4.16

3.4%

115%

Arsenic

127

136

1.89

1.4%

107%

Barium

698

718

23.6

3.3%

103%

Beryllium

78.3

80.5

2.90

3.6%

103%

Cadmium

86.7

85.4

2.71

3.2%

99%

Calcium

39519

40469

1524.6

3.8%

102%

Chromium

72.4

74.7

1.72

2.3%

103%

Cobalt

9.9

10.2

0.19

1.9%

103%

Copper

812

809

19.1

2.4%

100%

Iron

23934

24802

811.03

3.3%

104%

Lead

105

110

2.33

2.1%

104%

Magnesium

3261

3365

135

4.0%

103%

Manganese

558

595

16.0

2.7%

107%

Mercury

53.6

55.0

2.22

4.0%

103%

Molybdenum

96.5

92.7

2.71

2.9%

96%

Nickel

47.7

49.0

1.74

3.5%

103%

Potassium

4293

4279

117.7

2.8%

100%

Selenium

65.7

68.8

1.95

2.8%

105%

Silver

89.3

90.1

1.81

2.0%

101%

Sodium

2986

3177

96.17

3.0%

106%

Thallium

100

102

0.943

0.9%

102%

Vanadium

37.0

39.1

0.87

2.2%

106%

Zinc

821

758

24.2

3.2%

92%

Click here to download the Application Note in PDF format.

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4551 Zimmerman Ave
Niagara Falls, ON L2E 3M5
info@coldblock.ca.